Apparatus and process involved in chlorination.



A K. BROWN. .APPARATUS AND PROCESS INVOLVED'IN CHLORINATION.

APPLICATION FILED MAY17|I9I7 Patented Feb. 11,1919.

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K. BROWN. APPARATUS'AND PHocEss INVOLVED 1N cHLoRl-NATION.

APPLICATION FILED MAYI7. 19H. y 1116111611161). 11, 1919.

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'To all whom it may concern ntic.

"'{IRK- BROWN', 0F MONTCLAIR, N'EW JERSEY, ASSIGNOR T0 CONDENSITE COMPANY OF AMERICA, 0F BLOOMFIELD, NEW JERSEY, A CORPORATION 0F NEW JERSEY.

Tus A1111 rnocEss InvoLvEn IN cHLonINATIoN.

Be. it known that I, KIRK BROWN, 'a citi- .zen of the United States, .residing at Mont clair, in the county of Essex and State of New Jersey, have invented certain new and useful Improvements in Apparatus and ProcessesInvolved in Chlorination, of which the following is a specification. My invention relates to improvements apparatus designed for chlorinating naphthalene, or for carrying out other chemical operations in which vapors pass lfrom one reaction vessel to another,1 which vapors must be constantlymaintained in a heated condition. lIn such operations, there isalways the danger that the vapors will cool suiiciently to solidify and choke up the pipes and valves connecting the various pots or reaction vessels in the system. inven'- tionovercomes this diiiiculty by inclosing the valves and a considerable portion of the piping within the chlorinating or` reaction vessels, so that the actual passage between adjacent vessels is reduced to a few inches of pipe only.

In the `chlorination of naphthalene, for which the invention is 'chiefly designed, the process 'isjcarried out by passing chlorm gas successively through a series of pots or reaction vessels containing molten naphthalene. The chlorin gas, or hydrochloric acid gas, which results Afrom its reaction upon the naphthalene, carries with it the vapors of naphthalene in its passage from one pot Ato the next. It is necessary that communication between these pots should be shut olf from time to time, and, accordingly, in the usual system, the pots are connected by pipes, each of wmch is provided with a valve. To' prevent solidifying of the naphthalene vapors within the pipes and valve passages, steam-jacketing is ordinarily em-` ployed and this is both troublesome and expensive. These diiculties are entirely overcome by 'my invention in which the heating means for the pots or reaction vessels themselves are used to prevent fall of temperature inthe piping and valves. The greater part of the piping and the valves are entirely within thevessels, as stated, preferably adjacent to steam-jacketed surfaces of the pots. The short length of piping between adjacent pots need not be steam-jacketed because it may be kept suiiiciently warm by the heat from the adjacent pots, a simple connection between the pots belng sui- Specication of Letters Patent.

Patenten' ret. 11, 1ere.

Application mea may rz. 1917. serial Non 169,185.

cient to house the piping extending through the same.

Another feature of my invention relates to the recovery of naphthalene from the gases which are carried olf at the end of the chlorinating process, and the consequent cleaning of these gases for subsequent recovery, as described hereafter.

In order that a clearer understanding of my invention may be had, attention is heret by directed to the accompanying drawings -formmg part of this specification and illus- "trating certainembodiments of my invention. In the drawlngs, Figure l represents somewhat diagrammaticall-y va side elevaconnected for operation, Fig. 2 is an enlarged vertical section through the adjacent portions of a` pair of pots, and'Fig. 3 isa diagrammatic side elevation of a series of chlorinating pots with means for separating tion of a series of three chlorinating pots naphthalene from the gases at the end of the process. I

Referring to the drawings, the chlorinat-A lng pots are illustrated at 1, 2 and 3, it being understood that any desired number maybe used. VThese pots are steam-jacketed', preferably on the bottoms and about their sides, as indicated at 4, 5 and 6. Naphthalene or other material to be chlorinated is led into the system, preferably from one end, until the same stands in fluid condition at a desired level in all of the pots, after whichl chlorin gas is pumped through the system, preferably from the other end. In the drawings I have diagrammatically indicated a tank at 7, from which naphthalene such as 2 and 3'and.1 and 2, is made by a suitable pipe 12, which preferably is made in two sections, one in each pot, the ends of Which are joined by a union or coupling 13, which is flanged and is suitably secured to fianges 14 and 15 on the adjacent pots. The sections of pipe 12 may be secured to the coupling by providing coacting screwthreads 16, and the coupling 13 may be provided with a' suitable draw-0R plug 17.

Referring to Fig. 2, the pipe 12 extends within pot 2 horizontally and closely adjacent to the steam-jacketed bottom to its end 18. In the adjacent pot 3 the pipe 12 is provided with an elbow 19, from which rises a vertical pipe'20, providing a valve.seat at its upper end, above the normal level of the naphthalene. A valve is provided hav ing a part 21 to coact with this valve seat and to control the opening in the top of pipe This valve is entirely Within the pot 3 and 1s operated from the exterior of the pot by any suitable means, such as the valve stem 23 extending upwardlythrough a suit- .able gland in the cover, this valve stem being adapted to be raised' and lowered through the standard 24 in which itis screwthreaded by means of a hand-wheel 25.

Any'suitable form of valve may be used, .but I prefer the form of lift valve illustrated, in which the lower` end of stem 23 is provided with an enlarged and rounded portion 22, engaging in a suitable opening in valve 21, to forma universal connection of limited movement, so that the valve may seat itself on its seat without the necessity -of an exact alinement of pipe 20 and valve stem 23. It will be noted that pipe 20 is moved from any pot in any desired manner,

as by drawing the same off through connectionl27 which may also be used for the purpose of drawing off samples.

In the usual operation, chlorine gas entering pot 3 passes throu h the naphthalene therein, some of the lorin gas,v together with hydrochloric acid gas2 passing through the valve and pipe connectlons to pot 2, and some of the gas slmilarly passing through the valve and pipe connections in pot2 into pot 1L When the material in pot 3 has been chlor- .inated to a desired stage, the. supply of chlorin gas passing through pipe 10 is stopped, the valve 21 in pot 3 is closed and the chlorinated product removed from pot 3, after which the partiall chlorinated product in pots 1 and 2 may e blown over or otherwise transferred to-pots 2 and 3 and pot l refilled with naphthalene to be chlorinated, after whichthe operation may be repeated. Thel above is, of course, merely illustrative of the use of the apparatus.

Another part of my invention, as stated,

consists in the method and means of freeing the gas, after its passage through all the chlorinating pots of the system, from the naphthalene vapors which its carries. As stated, the gas passing from pot 3 to pot 2 and on through the 'series-of pots used carries naphthalene vapors Awith it. These can be removed by` passing the gas through a solvent for the naphthalene, at a temperature low enough to condense the naphthalene vapors. I prefer to use mono-chloronaphthalene for the Solvent, as this is a liquidat room temperatures, and when lit has absorbed as much naphthalene from the gases as is advisable, it can be transferred into one of the chlorinatng ots as a desirable starting material for t e chlorination process. c

In Figs. 1 and 2 the chlorinating'apparatus only is shown. In Fig. 3 I have indicated diagrammatically a series oftwo chloinating pots, 3 and' 2, similar to those already described, it being understood that as many steam-jacketed pots are used as is desirable. as before, and some chlorin gas, together with some hydrochloric acid gas from the reaction with the naphthalene, passes over through pipe 12 into pot 2. The gas which collects in the upper part of pot 2 contains a larger percentage of hydrochloric acid 'gas,

and in a suitably designed seriesofpots may be all hydrochloricacid gas at the end of the series.

This gas passes through valve 22 and pipe 12', into the-vessel or pot. 28, which is preferably cooled .by being water-jacketed, and contains liquid. chloro-naphthalene lwhich may be nmono-chloro-naphthalene 29. y This pot does not require the baffle plates 26, and 1t may be termed a scrubber. Pipe 12 should end at the point where it enters the scrubber, as otherwise the'naphthalene carried by the gas would deposit therein and chokel it up. The hydrochloric acid gas which rises from the surface of this monochloro-naphthalene is freed from the naphthalene carried over with it into the scrubber, and passes oft' at 30, in purifiedcondition, to be recovered. The successful opera.- tion of this system depends considerably upon bringing the hydrochloric -acid gas to the scrubber in its heated condition, so that it will not deposit its naphthalene untll it gets into the relatively cold scrubber.

The process is continued unt1l the liquid in the scrubber has absorbed enough naphthalene to be no longer freely uid, when it is' removed, and preferably transferred to *one or more of the chlorinating pots, the

scrubber 28 then being. refilledv with monochloro-naphthalene, or the'systeln beingl connected up with a reserve scrubber. l contents ofthe scrubber are preferably transferred to the chlorin'atingpots by blow- Chlorin gas enters pot 3 at 10- The pipe 31 having a connection 33, for admitting airfrom a blower for transferring the liquid to pots 2 and 3, the chlorin admission pipe 10 being closed. The chlorinating pots may be provided with sufficient excess capacity to enable them to receive this charge. The pot 2 is represented as provided with a conection 8 to a'naphthalene tank 7, in which u naphthalene is heated to liquefyv the same,

and a connection 341 to the blower, for transferring the contents of pot 2 to pot 1, whenthe latter is to be refilled.

One advantage ofA this method is that thereby the chlorinating pots may readily be filled with -`starting material when a chlorinated product higher than the mono is de- Y sired. With the method described, the monochloro naphthalene serves to prevent the loss of naphthalene, to clean. the hydrochloric acid gas produced, land to serve as a part of the starting material, for the chlorinating pots, after it has performed its function in the scrubbers.

1. In chemical apparatus, the combination of a pair of normally closed chlorinating vessels, closely adjacent to each other, means for-introducing material to bechlorinated into one of the same, a pipe connecting said vessels, having one end within the lower portion of said first vessel, an upwardly extendmg pipe entirely within the second vessel, connected therein with said first pipe, f. a valve at the lupper end of said second pipe,

means 4for operating the same from the exterlor of the vessel, to open and close the same, means for heatlng said vessels, and

means for introducing` chlorin into said lsecond vessel, substantially as set forth..

l2. In. chemical apparatus, the combination of a pair of normally closed reaction vessels, a pipe connecting the same, having one end within the lower portion of one vessel, and the other end within the other vessel,'th`e end last mentioned being provided with a valve seat, a valve coacting therewith, within said vessel, means for operating the same from the exterior of the vessel, and means for maintaining'said vessels in heated condition, said second vessel having an admission pipe leading into the same, substantiallyV as set forth.

3. In chemical apparatusq the combination of a pair of normally closed reaction vessels, a pipe connecting the lower portions of the same, having one end within the lower portion of one vessel, and having an upwardly extending portion within the second vessel, terminating in a valve seat, a valve adapted to seat on said valve seat, within said vessel, a valve stem extending therefrom to the exterior of the vessel, and

.means for maintaining the portions of said vessels in which the said lengths of piping .are arranged', in a heated condition, saidl second vessel having an admission pipe leading into the lower portion of the same, substantially as set forth.

4. In chemical apparatus, the combination cfa pair of normally closed steam-- jacketed reaction vessels, a coupling connecting the same, pipe sections connected with said coupling, and extending within said vessels adjacent to steam-jacketed surfaces thereof, to their o posite ends, a valve seat at`one of said en s, a valve therefor,

means for operating the valve from the ex'- terior of the vessel, and an admission pipe leadinginto said last-n-amed vessel, subtan- .tially as set forth.

5. In chemical apparatus, the combination of a series of vessels for chlorinating y for leadingI gas from the upper part of said last named vessel, means for supplying liquid chloro-naphthalene thereto, and means for supplying melted naphthalene to said chlorinating vessels, substantially asset forth.

Y,6. In chemical apparatus, the. combination of a pair of normally closed reaction vessels, means for heating the same,fa pipe connecting the'same having one end withln the upper part of one vessel and the other end within the lower part of the second vessel, a third vessel adapted to hold liquid, a pipe connecting the upper part of the second vessel with the lower part of the third vessel, valves in said pipes, a gas admisslon pipe leading into the lower part of the first vessel, a gas exit pipe leading from the upper part of the third vessel, means for first. and means for introducing -a different liquid into the third, substantially -as set forth.

This specification signed and witnessed this 10th day of May, 1917.'

KIRK BROWN.

Witnesses:

M. S. GANG,

I. McIN'rosH. 

